Abstract

Solidified floating organic drop microextraction was applied as a separation/preconcentration step prior to the electrothermal atomic absorption spectrometric (ETAAS) determination of ultra trace of antimony species. The method was based on the formation of an extractable complex between Sb(III) and ammonium pyrrolidinedithiocarbamate at pH ~ 5, while Sb(V) was remained in the aqueous phase. The antimony extracted into 1-undecanol was determined by ETAAS. Total antimony was determined after the reduction of Sb(V) to Sb(III) with potassium iodide and ascorbic acid. The amount of Sb(V) was determined from the difference of concentration of total antimony and Sb(III). Under the optimum conditions an enhancement factor of 437.5 and a detection limit of 5.0 ng L−1for the preconcentration of 25 mL of sample was achieved. The relative standard deviation at 300 ng L−1 of antimony was found to be 3.5 % (n = 6). The proposed method was successfully applied to the determination of antimony in tea, basil and natural water samples.

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